Sample injector with metering device balancing pressure differences in an intermediate valve state

Patent metadata

Field	Value
Publication number	US-11519884-B2
Application number	US-202016993070-A
Country	US
Kind code	B2
Filing date	Aug 13, 2020
Priority date	Jun 3, 2009
Publication date	Dec 6, 2022
Grant date	Dec 6, 2022

Abstract

A sample injector for use in a fluid separation system for separating compounds of a fluidic sample in a mobile phase, the sample injector comprising a switchable valve, a sample loop in fluid communication with the valve and configured for receiving the fluidic sample, a metering device in fluid communication with the sample loop and configured for introducing a metered amount of the fluidic sample on the sample loop, and a control unit configured for controlling switching of the valve to transfer the sample loop between a low pressure state and a high pressure state via an intermediate state and for controlling the metering device during the intermediate state to at least partially equilibrate a pressure difference in the sample loop between the low pressure state and the high pressure state.

First claim

The invention claimed is:

1. A method of operating a liquid chromatography system, the liquid chromatography system comprising a liquid chromatography column and an injection valve, the method comprising:
isolating a sample loop of the liquid chromatography system from a high-pressure fluidic path in fluid communication with the liquid chromatography column, wherein:
the high-pressure fluidic path is at a pump pressure,
the sample loop is in fluid communication with the injection valve and comprises a sample conveying device for loading a sample on the sample loop, and
a volume of the sample conveying device is defined by a cavity in which a movable element is slidably mounted;

using a control unit comprising a motor and encoder to configure the injection valve to transfer the sample loop between a low pressure state and a high pressure state via an intermediate state to equilibrate a pressure difference in the sample loop between the low pressure state and the high pressure state; and
while the sample loop is isolated from the high-pressure fluidic path, decreasing the volume of the sample conveying device by sliding the movable element within the cavity from a first position to a second position to increase a pressure in the sample loop from the low pressure state at an essentially ambient pressure to the high pressure state at the pump pressure.

2. The method of claim 1 , wherein the injection valve comprises a rotary valve having a PRESSURE COMPENSATION position associated with the intermediate state, and wherein, in this position:
(i) first and second sample loop ports of the injection valve are closed so as to facilitate a pressurization of the sample loop, and
(ii) first and second high-pressure ports of the injection valve are connected so as to operatively connect a high-pressure pump in fluid communication with the high-pressure fluidic path to the liquid chromatography column.

3. The method of claim 2 , in which the sample loop includes a first connecting piece and a second connecting piece, in which the first connecting piece is connected to the first sample loop port of the injection valve and to the sample conveying device, in which the second connecting piece is connected to the second sample loop port of the injection valve and to the sample conveying device, in which the second connecting piece includes an intake segment and a feed segment, in which the intake segment and the feed segment are configured to be separated.

4. The method of claim 1 , further comprising placing the injection valve in the PRESSURE COMPENSATION position by rotating a rotor of the injection valve with respect to a stator of the injection valve.

5. The method of claim 1 further comprising using the motor and encoder to operate the injection valve to connect the sample loop to the high-pressure fluidic path such that the pump pressure from a high-pressure pump of the liquid chromatography system is applied to the sample loop, and a sample in the sample loop flows from the sample loop into the high-pressure fluidic path and to the chromatography column.

6. The method of claim 5 further comprising:
after operating the injection valve to connect the sample loop, introducing the sample into the chromatography column;
after introducing the sample into the chromatography column, using the motor and encoder to disconnect the sample loop from the high-pressure fluidic path by placing the injection valve in a pressure compensation position; and
increasing the volume of the sample conveying device to reduce the pressure in the sample loop from the pump pressure of the liquid chromatography column to the essentially ambient pressure.

7. The method of claim 1 , in which the moveable element includes a plunger.

8. A method of injecting a sample in a liquid chromatography system, the method comprising:
using a motor and encoder to isolate a sample loop of the liquid chromatography system from a high-pressure fluidic path of the liquid chromatography system, the high-pressure fluidic path at a pump pressure in fluid communication with a liquid chromatography column of the liquid chromatography system, wherein the sample loop is in fluid communication with a sample conveying device for loading a sample on the sample loop, wherein a volume of the sample conveying device is defined by a cavity in which a movable element is slidably mounted;
placing the sample in the sample loop;
with the sample placed in the sample loop and with the sample loop remaining isolated from the high-pressure fluidic path, decreasing the volume of the sample conveying device by moving the movable element within the cavity from a first position to a second position to increase a pressure in the sample loop from an essentially ambient pressure to essentially correspond to the pump pressure of the high-pressure fluidic path; and
using the motor and encoder to connect the sample loop to the high-pressure fluidic path so that the pump pressure from a high-pressure pump is applied to the sample loop to cause the sample in the sample loop to flow from the sample loop through a portion of the high-pressure fluidic path to the chromatography column.

9. The method of claim 8 further including:
after the sample has flowed into the high-pressure fluidic path, isolating the sample loop from the high-pressure fluidic path of the liquid chromatography system; and
increasing the volume of the sample conveying device to reduce the pressure in the sample loop to the essentially ambient pressure.

10. The method of claim 8 , wherein isolating the sample loop from the high-pressure loop includes placing an injection valve in a PRESSURE COMPENSATION position in which
first and second sample loop ports of the injection valve are closed so as to facilitate pressurization of the sample loop, and
first and second high-pressure ports of the injection valve are connected so as to operatively connect the high-pressure pump to the liquid chromatography column.

11. The method of claim 10 wherein placing the injection valve in the PRESSURE COMPENSATION position includes using the motor to rotate a rotor of the injection valve with respect to a stator of the injection valve.

12. The method of claim 10 , in which the sample loop includes a first connecting piece and a second connecting piece, in which the first connecting piece is connected to the first sample loop port of the injection valve and to the sample conveying device, in which the second connecting piece is connected to the second sample loop port of the injection valve and to the sample conveying device, in which the second connecting piece includes an intake segment and a feed segment, in which the intake segment and the feed segment are configured to be separated.

13. The method of claim 8 wherein the movable element is connected to a drive device which is operable to move the movable element within the cavity.

14. The method of claim 8 , in which the moveable element includes a plunger.

15. A method of operating a liquid chromatography system, the liquid chromatography system comprising a liquid chromatography column and an injection valve, the method comprising:
isolating a sample loop of the liquid chromatography system from a high-pressure fluidic path in fluid communication with the liquid chromatography column, wherein the high-pressure fluidic path is at a pump pressure, the sample loop is in fluid communication with the injection valve, the sample loop comprises a sample conveying device for loading a sample on the sample loop and having a syringe and a moveable element within the syringe, and isolating the samp

Assignees

• Agilent Technologies Inc

Inventors

• Glatz Bernd
• Kretz Wolfgang

Classifications

• G01N30/36

  in high pressure liquid systems · CPC title

• G01N30/20 Primary

  using a sampling valve · CPC title

• G01N2030/207

  with metering cavity, e.g. sample loop · CPC title

• G01N30/32

  of pressure or speed (G01N30/36 takes precedence) · CPC title

• G01N2030/027

  Liquid chromatography · CPC title